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Phthalate hydrogenation catalyst, preparation method thereof and application of catalyst

A phthalate, hydrogenation catalyst technology, applied in the preparation of carboxylate, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of affecting catalyst utilization efficiency and selectivity , the low accessibility of phthalates, the high dispersion of catalyst active components, etc., to achieve the effects of high product yield, low loading, and mild reaction conditions

Inactive Publication Date: 2019-07-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the prior art and the above-mentioned two kinds of phthalate hydrogenation catalysts all use a single carrier, the high dispersion of catalyst active components is limited, especially the active components in micropores or smaller nanopores are very important for o-phthalates. Diformate esters are less accessible, affecting catalyst utilization efficiency and selectivity

Method used

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  • Phthalate hydrogenation catalyst, preparation method thereof and application of catalyst
  • Phthalate hydrogenation catalyst, preparation method thereof and application of catalyst
  • Phthalate hydrogenation catalyst, preparation method thereof and application of catalyst

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preparation example Construction

[0035] The preparation method of above-mentioned phthalate hydrogenation catalyst comprises the following steps:

[0036] (1) Add the first carrier of 100-200 mesh and the second carrier of 200-400 mesh into the ball mill according to the metering, carry out ball milling for 5-10 hours, and mix well;

[0037] (2) Dry the mixed composite carrier at 110°C-120°C for 12-24 hours;

[0038] (3) Take an aqueous solution of alkaline earth metal nitrate compound to impregnate the composite carrier with equal volume, then dry at 100-140°C for 10-24 hours, and bake at 400-500°C for 2-6 hours under an inert atmosphere;

[0039] (4) Dissolving ruthenium trichloride in deionized water or alcohol is configured into an aqueous solution or an alcohol solution, and saturating and impregnating the composite carrier after the above-mentioned loading aid with the solution to form a catalytic matrix;

[0040] (5) Dry the catalyst precursor at 20°C-40°C for 12-24 hours, and then at 110°C-120°C for ...

Embodiment 1

[0047] Weigh 3g of fruit shell activated carbon, grind and sieve to get 100-200 mesh, weigh 2g200-400 mesh ZrO2, add activated carbon and ZrO2 to a planetary ball mill (Nanjing Chishun Technology Development Co., Ltd., XQM-2L), and turn at 200 rpm Perform ball milling and mixing within a range of 10 hours per minute; the mixed composite carrier is dried at 120° C. for 12 hours. Take 0.1037 g of anhydrous ruthenium trichloride and dissolve it in deionized water, add it to the dried composite carrier, stir evenly, dry at room temperature for 12 hours, and dry at 120° C. for 12 hours. Then, the catalyst precursor impregnated with active components was calcined at 300° C. for 4 h in a nitrogen atmosphere. Catalyst A was obtained after reduction at 200° C. for 3 h in a hydrogen atmosphere (0.05-0.15 MPa), wherein the active component accounted for 1% of the total mass of the carrier.

[0048] Using 2.5g of di-isooctyl phthalate as raw material and 25g of ethanol as solvent, weigh ...

Embodiment 2

[0050] Weigh 6g of coconut shell activated carbon, grind and sieve to take 100-200 mesh, weigh 4g of 200-400 mesh SiO2, add activated carbon and SiO2 to a ball mill, and perform ball milling and mixing for 10 hours; the mixed composite carrier is extruded into strips, ground Sieve 20-40 mesh and dry at 140°C for 12h. 0.2074 g of anhydrous ruthenium trichloride was dissolved in deionized water, added to the dried carrier, stirred evenly, dried at room temperature for 12 hours, and dried at 140°C for 12 hours. Calcined at 400°C for 4h in a nitrogen (0.1-0.15MPa) atmosphere. Catalyst B was obtained after reduction at 200° C. for 4 h in a hydrogen atmosphere (0.05-0.15 MPa), wherein the active component accounted for 1% of the total mass of the carrier.

[0051] Using 2.5g of di-isooctyl phthalate as raw material and 25g of ethanol as solvent, weigh 0.5g of catalyst B, and react for 4 hours at a reaction temperature of 120°C, an initial hydrogen pressure of 5.0MPa, and a stirring...

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Abstract

The invention relates to a phthalate hydrogenation catalyst which is characterized by comprising an active component, a composite support and auxiliaries, wherein the active component comprises ruthenium chloride, the composite support comprises a first support and a second support, the first support is optional one or two of shell activated carbon or coconut shell activated carbon, and the secondsupport is optional one or two of SiO2, ZrO2 or TiO2. The activated carbon and solid oxide composite support is used for supporting precious metal Ru and provided with activated carbon micropores andmesopores in solid oxide, so that a microporous-mesoporous hierarchical pore structure is formed, high dispersion of the active component is facilitated, diffusion of reactants can be improved, and the use efficiency of the catalyst is improved. The transformation rate of the catalyst in reaction of cyclohexane phthalate preparation by phthalate hydrogenation is 100%, and cyclohexane phthalate selectivity reaches up to 99.9%. The catalyst is simple in preparation technology, the support is low in price and easy to obtain, the active component is low in precious metal loading capacity, the catalyst is high in activity and product yield, by-products are almost avoided, reaction conditions are mild, and reaction can be performed under lower pressure and at lower temperature.

Description

technical field [0001] The invention relates to the technical field of hydrogenation catalyst preparation, in particular to a phthalate hydrogenation catalyst and its preparation method and application. Background technique [0002] 1,2-Cyclohexane dicarboxylate is a kind of environmentally friendly plasticizer that can be used in PVC processing and manufacturing toys, medical equipment, and food packaging. It has the characteristics of hygiene and low toxicity. At present, domestic plasticizers are mainly phthalate plasticizers, but they are extremely harmful to the environment, polluting air, soil, water and even food, and then accumulate in the human body through bioaccumulation and amplification , endangering human health. Studies have shown that once phthalates enter the human body, they will quickly accumulate in adipose tissue, which is not easy to excrete, and will interfere with the body's endocrine system, affect hormone levels, and may lead to hypofunction of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J23/58C07C67/303C07C69/75
CPCB01J23/462B01J23/58C07C67/303C07C2601/14C07C69/75
Inventor 赵玉军徐艳王岩吴晨光
Owner TIANJIN UNIV
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